US6599594B1 - Glass container for medicinal purposes - Google Patents

Glass container for medicinal purposes Download PDF

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US6599594B1
US6599594B1 US09/564,758 US56475800A US6599594B1 US 6599594 B1 US6599594 B1 US 6599594B1 US 56475800 A US56475800 A US 56475800A US 6599594 B1 US6599594 B1 US 6599594B1
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weight
glass container
fluorine
coating
equal
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US09/564,758
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US20030134060A1 (en
Inventor
Marten Walther
Andreas Geiger
Petra Auchter-Krummel
Michael Spallek
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Schott AG
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Schott Glaswerke AG
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/04Coating on selected surface areas, e.g. using masks
    • C23C16/045Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/30Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/28Other inorganic materials
    • C03C2217/282Carbides, silicides
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/15Deposition methods from the vapour phase
    • C03C2218/152Deposition methods from the vapour phase by cvd
    • C03C2218/153Deposition methods from the vapour phase by cvd by plasma-enhanced cvd
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S215/00Bottles and jars
    • Y10S215/03Medical
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/13Hollow or container type article [e.g., tube, vase, etc.]
    • Y10T428/131Glass, ceramic, or sintered, fused, fired, or calcined metal oxide or metal carbide containing [e.g., porcelain, brick, cement, etc.]
    • Y10T428/1317Multilayer [continuous layer]
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/13Hollow or container type article [e.g., tube, vase, etc.]
    • Y10T428/131Glass, ceramic, or sintered, fused, fired, or calcined metal oxide or metal carbide containing [e.g., porcelain, brick, cement, etc.]
    • Y10T428/1317Multilayer [continuous layer]
    • Y10T428/1321Polymer or resin containing [i.e., natural or synthetic]

Definitions

  • the present invention relates to a glass container for medicinal purposes, and, more particularly, to a glass container for storing and preserving pharmaceutical or diagnostic solutions for medicinal purposes, which is provided with an anti-adherent coating on its interior surface or surfaces.
  • Glass containers for medicinal purposes i.e. containers having pharmaceuticals or diagnostics as contents
  • containers having pharmaceuticals or diagnostics as contents are on the market in a most wide variety of embodiments, in order to take into account their respective purposes, associated administration forms and the respective contents.
  • Glass containers for medicinal contents should have interior surfaces which have the least possible adherence for their contents, i.e. as large as possible a wetting angle for aqueous contents, in order to permit a complete emptying of residues from the container. This is particularly true for comparatively small glass containers with very expensive contents.
  • silicone oil is dispensed from the surfaces and that the silicone oil may be introduced into human or animal bodies. Furthermore undesirable adsorption phenomena occur on the silicone-coated surface. Protein binding is one of the undesirable adsorption phenomena and is particularly notable. Furthermore heavy metal impurities are unavoidably present in the silicone oil. Thus suitable expensive testing is prescribed In European formularies. Furthermore auxiliary substances (eg. detergents), which must be used for stabilizing silicone emulsions, are critical.
  • a glass container for storing and preserving pharmaceutical or diagnostic solutions for medicinal purposes comprising a container closure device and an amorphous, transparent and pharmaceutically acceptable anti-adherent coating provided on the entire interior surface of the glass container over the entire interior surface up to the closure device, and wherein the anti-adherent coating has a contact angle for wetting with water of ⁇ 80°, even after autoclaving at about 120° C. for about 20 min, contains the elements Si, O, C and H and is deposited by means of a plasma-enhanced chemical vapor deposition method (PECVD), preferably by means of a plasma-pulsed, chemical vapor deposition method (PICVD).
  • PECVD plasma-enhanced chemical vapor deposition method
  • PICVD plasma-pulsed, chemical vapor deposition method
  • Medicinal glass containers of this type i.e. according to the invention, have interior surfaces that to a large extent reject water or wetting with water, which permits a nearly complete emptying of the container. It also has the great medically related advantage that no silicone substances are introduced into the pharmaceutical or diagnostic contents and thus into the human body.
  • the anti-adherent layer or coating according to the invention is equal to typical pharmaceutical stress test conditions, e.g. typical sterilization conditions, without loosing its function.
  • the glass container according to the invention is thus to a large extent pharmaceutically acceptable.
  • the anti-adherent layer comprises at least 1% by weight silicon and at least 5% by weight carbon.
  • the hydrophobic properties of the coating can be augmented, when the anti-adherent coating contains fluorine according to a further embodiment of the invention.
  • FIGURE is a partially side, partially cutaway cross-sectional view through a glass container for medicinal purposes according to the invention.
  • the sole FIGURE shows a glass container 1 for medicinal purposes in a configuration suitable for a typical application, which is provided with a conventional closure device 2 .
  • the glass container 1 serves for storage and preservation of a pharmaceutical or diagnostic solution 5 .
  • the glass container 1 is preferably made from a glass type I according to German Dispensatory, 10th Edition, corresponding to a borosilicate glass.
  • the particular glass type mentioned above and the.shape of the glass bottle are features of preferred embodiments.
  • the glass bottle may also have other shapes and can be made from other types of glass, which have the required properties for other applications.
  • Especially the glass bottle may be made from glass of a lower hydrolytic class, especially the so-called neutral glass.
  • the interior of the glass bottle should reject water to a large extent. That means that it should have as large as possible a wetting angle for its aqueous contents 5 , especially in order to permit complete emptying so as to minimize any residue left in the bottle. This is also true for a comparatively small glass container with very expensive contents.
  • a special coating 4 is provided over the whole interior surface of the wall 3 of the glass bottle 1 .
  • This coating comprises an anti-adherent layer with a contact angle for water of ⁇ 80°, which is pharmaceutically acceptable, i.e. free of heavy metals and stable under the usual test conditions, especially autoclaving for 20 minutes at 121° C. and/or in hot air sterilization for 30 minutes at 300° C.
  • the layer is amorphous, clear and transparent and contains the elements Si, O, C and H, with silicon content of at least 1% by weight and a C content of at least 5% by weight.
  • the layer 4 also contains fluorine, whose content is in a reciprocal relationship to the carbon content.
  • the coating or layer 4 is produced bymeans of a plasma-enhanced chemical vapor deposition process (PECVD).
  • PECVD plasma-enhanced chemical vapor deposition process
  • a plasma-assisted layer deposition from the gas phase occurs, in which the layer material is supplied in the form of so-called precursor gases.
  • precursor gases are broken down with the required energy being supplied to the system by electrical high frequency plasma, particularly in a plasma-pulsed chemical vapor deposition process (PICVD).
  • the container for medical purposes according to the present invention has the following properties:
  • PFCVD reactor Glass containers in the form of glass bottles are placed in a PFCVD reactor, whose structure corresponds principally to that disclosed in DE 44 38 359 A1.
  • a gas nozzle device extends into the mouth of the bottle.
  • the reactor is evacuated to 0.05 mbar by a pump.
  • CF 3 C 6 F 10
  • HMDEO hexamethyldisiloxane
  • RF power is coupled to an electrode in the reactor inductively by means of coils through a matching network and Ignites plasma in the reactor.
  • the entire apparatus is arranged within an electrical shielding. In this process the reaction gas is converted into a coating in the whole bottle at about 300 W HF power (13.56 MHz).
  • a contact angle of 95° to 102° (relative to water) is produced in all bottles by this process. This contact angle becomes 85° to 95° during autoclaving at. 121° C. for 20 minutes. All bottles were filled with an aqueous.suspension. After a storage time of 1 week the pouring behavior was tested. In contrast to the uncoated bottles, in which a residue of flecks of the suspension remained over the entire interior surface after emptying the bottles, the bottles coated in the above-described manner according to the invention, could be completely emptied without leaving a residue.
  • Glass containers in the form of glass bottles are placed in a PICVD reactor, whose structure corresponds principally to that disclosed in DE 196 29 877 C1.
  • the reactor is evacuated to 0.9 mbar by a pump.
  • a gas mixture comprising 10 sccm HMDSO, 5 sccm O 2 and 2 sccm C 6 F 6 is supplied by a supply device.
  • Pulsed power was provided at 2.45 GHz by a microwave discharge source, which ignites a plasma in the glass bottle. After deposition of a 30 nm layer the microwave power is turned off and the bottles are aerated.
  • the tests found that after the coating is formed the contact angle for water was 91° to 105°. This contact angle is reduced about 6° on average after autoclaving. This behavior of a watery suspension that is poured out of bottles coated in this manner is similar to that described in connection with the previous PECVD method.
  • German Patent Application 199 21 303.8 of May 7, 1999 is incorporated here by reference.
  • This German Patent Application describes the invention described hereinabove and claimed in the claims appended hereinbelow and provides the basis for a claim of priority for the instant invention under 35 U.S.C. 119.

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  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Medical Preparation Storing Or Oral Administration Devices (AREA)
  • Details Of Rigid Or Semi-Rigid Containers (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The glass container stores and preserves pharmaceutical or diagnostic solutions for medicinal purposes. So that the container is free of silicones and other residues, it is provided with an amorphous, transparent anti-adherent coating (4) over its entire interior surface from its bottom over the wall (3) to the closure device (2). This anti-adherent coating (4) is free of heavy metals, free of silicones, is stable after autoclaving at about 120° C. for about 20 min or hot air sterilization for 30 min at 300° C., has a contact angle for wetting with water of ≧80°, contains silicon, oxygen, carbon, fluorine and hydrogen and is deposited by a PECVD method, especially a PICVD method. If the coating contains less than 0.1% by weight fluorine, then it contains greater than or equal to 10% by weight carbon, but if it contains greater than or equal to 0.1% fluorine then it contains greater than or equal to 5% by weight carbon.

Description

BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a glass container for medicinal purposes, and, more particularly, to a glass container for storing and preserving pharmaceutical or diagnostic solutions for medicinal purposes, which is provided with an anti-adherent coating on its interior surface or surfaces.
2. Prior Art
Glass containers for medicinal purposes, i.e. containers having pharmaceuticals or diagnostics as contents, are on the market in a most wide variety of embodiments, in order to take into account their respective purposes, associated administration forms and the respective contents.
Glass containers for medicinal contents should have interior surfaces which have the least possible adherence for their contents, i.e. as large as possible a wetting angle for aqueous contents, in order to permit a complete emptying of residues from the container. This is particularly true for comparatively small glass containers with very expensive contents.
Glass containers for medicinal purposes have been treated with silicone oils (polydimethylsiloxane oil) or silicone oil emulsions, in order to produce anti-adherent interior surfaces. This has been disclosed in U.S. Pat. No. A 2,504,482, among other prior art references. This method is also described in European medical formularies.
The main disadvantage of this method is that silicone oil is dispensed from the surfaces and that the silicone oil may be introduced into human or animal bodies. Furthermore undesirable adsorption phenomena occur on the silicone-coated surface. Protein binding is one of the undesirable adsorption phenomena and is particularly notable. Furthermore heavy metal impurities are unavoidably present in the silicone oil. Thus suitable expensive testing is prescribed In European formularies. Furthermore auxiliary substances (eg. detergents), which must be used for stabilizing silicone emulsions, are critical.
Methods for modification of the interior surfaces of the glass container using silanes, silazanes, etc, are known (GB 2,230,260 A) as well as by application of silicone oil. A monolayer is deposited on the surfaces from the liquid or gas phase after an expensive cleaning process, which often uses reactive acids, such as chromo-sulfuric acid, etc.
This process has the disadvantage that a fresh expensive washing process is required after the surface treatment, in order to remove the residual chemicals most completely. Furthermore no silane or silanized layers, which resist the action of the typical pharmaceutical tests sufficiently, which especially withstand autoclaving at 121° C. for 20 minutes, are currently known.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a glass container for medicinal purpose of the above-described kind, so that its interior surface has an outstanding anti-adherent property, it is equal to the typical pharmaceutical stress test conditions and it introduces nosilicone into the solution found in the glass container.
According to the invention this object is attained with a glass container for storing and preserving pharmaceutical or diagnostic solutions for medicinal purposes, comprising a container closure device and an amorphous, transparent and pharmaceutically acceptable anti-adherent coating provided on the entire interior surface of the glass container over the entire interior surface up to the closure device, and wherein the anti-adherent coating has a contact angle for wetting with water of ≧80°, even after autoclaving at about 120° C. for about 20 min, contains the elements Si, O, C and H and is deposited by means of a plasma-enhanced chemical vapor deposition method (PECVD), preferably by means of a plasma-pulsed, chemical vapor deposition method (PICVD).
Medicinal glass containers of this type, i.e. according to the invention, have interior surfaces that to a large extent reject water or wetting with water, which permits a nearly complete emptying of the container. It also has the great medically related advantage that no silicone substances are introduced into the pharmaceutical or diagnostic contents and thus into the human body.
Tests have shown that the anti-adherent layer or coating according to the invention is equal to typical pharmaceutical stress test conditions, e.g. typical sterilization conditions, without loosing its function. The glass container according to the invention is thus to a large extent pharmaceutically acceptable.
Preferably the anti-adherent layer comprises at least 1% by weight silicon and at least 5% by weight carbon. The hydrophobic properties of the coating can be augmented, when the anti-adherent coating contains fluorine according to a further embodiment of the invention.
According to a preferred embodiment of the invention the percentage content of fluorine in the anti-adherent layer is related to the percentage content of carbon by the following reciprocal relationship:
When fluorine<0.1% by weight, then C≧10% by weight;
When F≧0.1% by weight, then C≧5% by weight.
BRIEF DESCRIPTION OF THE DRAWING
The objects, features and advantages of the invention will now be illustrated in more detail with the aid of the following description of the preferred embodiment, with reference to the accompanying sole FIGURE which is a partially side, partially cutaway cross-sectional view through a glass container for medicinal purposes according to the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The sole FIGURE shows a glass container 1 for medicinal purposes in a configuration suitable for a typical application, which is provided with a conventional closure device 2. The glass container 1 serves for storage and preservation of a pharmaceutical or diagnostic solution 5.
The glass container 1 is preferably made from a glass type I according to German Dispensatory, 10th Edition, corresponding to a borosilicate glass. The particular glass type mentioned above and the.shape of the glass bottle are features of preferred embodiments. According to the invention the glass bottle may also have other shapes and can be made from other types of glass, which have the required properties for other applications. Especially the glass bottle may be made from glass of a lower hydrolytic class, especially the so-called neutral glass.
It is desirable that the interior of the glass bottle should reject water to a large extent. That means that it should have as large as possible a wetting angle for its aqueous contents 5, especially in order to permit complete emptying so as to minimize any residue left in the bottle. This is also true for a comparatively small glass container with very expensive contents.
In order to achieve this behavior, a special coating 4 is provided over the whole interior surface of the wall 3 of the glass bottle 1. This coating comprises an anti-adherent layer with a contact angle for water of ≧80°, which is pharmaceutically acceptable, i.e. free of heavy metals and stable under the usual test conditions, especially autoclaving for 20 minutes at 121° C. and/or in hot air sterilization for 30 minutes at 300° C. The layer is amorphous, clear and transparent and contains the elements Si, O, C and H, with silicon content of at least 1% by weight and a C content of at least 5% by weight. Preferably the layer 4 also contains fluorine, whose content is in a reciprocal relationship to the carbon content. In other words,
when fluorine<0.1% by weight, then C≧10% by weight;
when F≧0.1% by weight, then C≧5% by weight.
The coating or layer 4 is produced bymeans of a plasma-enhanced chemical vapor deposition process (PECVD). In this process a plasma-assisted layer deposition from the gas phase occurs, in which the layer material is supplied in the form of so-called precursor gases. These pre-cursor gases are broken down with the required energy being supplied to the system by electrical high frequency plasma, particularly in a plasma-pulsed chemical vapor deposition process (PICVD).
These processes and their associated apparatus are well known. Examples are described in DE 196 29 877 C1 and DE 44 38 359 A1, which were produced by the present applicant.
The container for medical purposes according to the present invention has the following properties:
a) its interior surface rejects water, so that its aqueous contents have the greatest possible wetting angle with its interior surface, in order to obtain complete emptying without leaving any residue;
b) its interior surface does not bind proteins;
c) its interior surface is free of silicone (polydimethylsiloxanes);
d) it is stable during typical pharmaceutical stress test conditions and/or terminal sterilization (autoclaving in steam at 121° C. for 20 minutes);
e) it has a high degree of transparency;
f) it has a high stability against washing processes, drying processes, hot air sterilization, filling processes and closing processes, including a washing process with hot distilled water arid a hot air sterilization with temperatures up to 300° C. and dwell times of up to 30 minutes;
g) it provides a high degree of chemical purity, i.e. it is not necessary to use solvents and/or aggressive chemicals for surface activation or cleaning; and it may be produced by a simple method.
It has been surprisingly found that not only the adherence of particles in aqueous suspensions on container interior surfaces is drastically reduced, but also that this is also true for suspensions, which contain an inert propellant gas, such as e.g. R134a, R127. This is also true for alcoholic suspensions.
EXAMPLES
The following two examples which are representative of numerous other tests are described in the following paragraphs. These examples show that the glass container according to the invention has properties that are superior to those of the prior art.
Example 1 Coating According to a PECVD Method
Glass containers in the form of glass bottles are placed in a PFCVD reactor, whose structure corresponds principally to that disclosed in DE 44 38 359 A1. A gas nozzle device extends into the mouth of the bottle. The reactor is evacuated to 0.05 mbar by a pump. Then a mixture of C6F10(CF3)2 and 5 sccm of hexamethyldisiloxane (HMDEO) is conducted into the bottle through the gas nozzle device. RF power is coupled to an electrode in the reactor inductively by means of coils through a matching network and Ignites plasma in the reactor. The entire apparatus is arranged within an electrical shielding. In this process the reaction gas is converted into a coating in the whole bottle at about 300 W HF power (13.56 MHz).
A contact angle of 95° to 102° (relative to water) is produced in all bottles by this process. This contact angle becomes 85° to 95° during autoclaving at. 121° C. for 20 minutes. All bottles were filled with an aqueous.suspension. After a storage time of 1 week the pouring behavior was tested. In contrast to the uncoated bottles, in which a residue of flecks of the suspension remained over the entire interior surface after emptying the bottles, the bottles coated in the above-described manner according to the invention, could be completely emptied without leaving a residue.
Example 2 Coating According to a PICVD Method
Glass containers in the form of glass bottles are placed in a PICVD reactor, whose structure corresponds principally to that disclosed in DE 196 29 877 C1. The reactor is evacuated to 0.9 mbar by a pump. In these bottles a gas mixture comprising 10 sccm HMDSO, 5 sccm O2 and 2 sccm C6F6 is supplied by a supply device. Pulsed power was provided at 2.45 GHz by a microwave discharge source, which ignites a plasma in the glass bottle. After deposition of a 30 nm layer the microwave power is turned off and the bottles are aerated. The tests found that after the coating is formed the contact angle for water was 91° to 105°. This contact angle is reduced about 6° on average after autoclaving. This behavior of a watery suspension that is poured out of bottles coated in this manner is similar to that described in connection with the previous PECVD method.
The disclosure in German Patent Application 199 21 303.8 of May 7, 1999 is incorporated here by reference. This German Patent Application describes the invention described hereinabove and claimed in the claims appended hereinbelow and provides the basis for a claim of priority for the instant invention under 35 U.S.C. 119.
While the invention has been illustrated and described as embodied in a glass container for medicinal purposes, it is not intended to be limited to the details shown, since various modifications and changes may be made without departing in any way from the spirit of the present invention.
Without further analysis, the foregoing will so fully reveal the gist of the present invention that others can, by applying current knowledge, readily adapt it for various applications without omitting features that, from the standpoint of prior art, fairly constitute essential characteristics of the generic or specific aspects of this invention.
What is claimed is new and is set forth in the following appended claims:

Claims (3)

We claim:
1. A glass container for storing and preserving pharmaceutical or diagnostic solutions for medicinal purposes, wherein said glass container comprises a closure device (2) and an amorphous, transparent anti-adherent coating (4) provided on an entire interior surface thereof over the entire interior surface up to the closure device;
wherein the anti-adherent coating is free of heavy metals, is free of silicones, is stable after autoclaving at about 120° C. for about 20 min or hot air sterilization for 30 min at 300° C., has a contact angle for wetting by water of ≧80°, even after said autoclaving at about 120° C. for about 20 min, and wherein the anti-adherent coating contains silicon, oxygen, fluorine, carbon and hydrogen and is deposited by means of a plasma-enhanced chemical vapor deposition process;
wherein said coating contains greater than or equal to 10 percent by weight of said carbon when said coating contains less than 0.1 percent by weight of said fluorine, but said coating contains greater than or equal to 5 percent by weight of said carbon when said coating contains greater than or equal to 0.1 percent by weight of said fluorine.
2. The glass container as defined in claim 1, wherein said plasma-enhanced chemical vapor deposition process is a plasma-pulsed chemical vapor deposition process.
3. The glass container as defined in claim 1, wherein said anti-adherent coating (4) contains at least 1% by weight of said silicon.
US09/564,758 1999-05-07 2000-05-04 Glass container for medicinal purposes Expired - Lifetime US6599594B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19921303 1999-05-07
DE19921303A DE19921303C1 (en) 1999-05-07 1999-05-07 Medical glass container, for holding pharmaceutical or medical diagnostic solution, has an inner PECVD non-stick layer containing silicon, oxygen, carbon and hydrogen
DE19921303.8-45 1999-05-07

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US20030134060A1 US20030134060A1 (en) 2003-07-17
US6599594B1 true US6599594B1 (en) 2003-07-29

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EP (1) EP1050517B1 (en)
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DE (2) DE19921303C1 (en)
HK (1) HK1032776A1 (en)

Cited By (64)

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US20040199138A1 (en) * 2001-07-21 2004-10-07 Mcbay William Edward Storage of liquid compositions
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